CN103131319A - Bi-component nanometer polyaniline-epoxy acrylic resin/polyurethane interpenetrating network electric conduction and antistatic coating and preparation method - Google Patents
Bi-component nanometer polyaniline-epoxy acrylic resin/polyurethane interpenetrating network electric conduction and antistatic coating and preparation method Download PDFInfo
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- CN103131319A CN103131319A CN 201110387930 CN201110387930A CN103131319A CN 103131319 A CN103131319 A CN 103131319A CN 201110387930 CN201110387930 CN 201110387930 CN 201110387930 A CN201110387930 A CN 201110387930A CN 103131319 A CN103131319 A CN 103131319A
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Abstract
The invention discloses a bi-component nanometer polyaniline-epoxy acrylic resin/polyurethane interpenetrating network electric conduction and antistatic coating and a preparation method. Under the action of an initiating agent and a catalytic agent, a nanometer polyaniline-epoxy acrylic resin compound A undergoes a chemical polymerization reaction with a castor oil polyurethane prepolymer B which contains isocyanate end groups, so that an electric conduction interpenetrating network polymer coating is formed. The A component is obtained through in-situ emulsion polymerization of phenylamine in epoxy acrylic resin, the A component is purified, dried, and added with an allyl monomer, a catalyst, a polymerization inhibitor, a light stabilizer and the like, and then the mixture is evenly stirred, and the B component is obtained through evenly mixing reactant which is obtained after castor oil reacts with diisocyanate and is added with a stabilizing agent. The coating is simple in preparing technology, convenient in operation, suitable for industrialized mass production, high in solid content and stable in conductivity, mechanical property, chemical corrosion resistance and environmental performance, so that the coating can be widely used in the fields such as electronic machines, electrostatic dust prevention floors and bridges.
Description
Technical field
The invention belongs to conductive polymer in macromolecular material, antistatic coating.Relate to two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network conduction antistatic coating and preparation method.
Background technology
Electrically conducting coating is to be applied on the macromolecular material of high resistivity, and a kind of functional special coating that makes it to have conduction current and get rid of the accumulate static charge ability can be coated on the surperficial or inner of any shape substrate.Electrically conducting coating is widely used in electronics, building, aviation and the field such as military at present, has easy construction, equipment is simple, with low cost and the plurality of advantages such as applied range.
People are in triturating, finding that polyaniline has conducts electricity very well, stable in the air and thermostability is high, and quality is light, synthesis technique is simple, preparation during electrically conducting coating with polyaniline as a kind of comparatively desirable conductive additive, when addition is the 5-8% polyaniline in electrically conducting coating, conductive filler material when its conductive effect is equivalent to increase by 40% in coating.
At present, polyaniline-conducting polymer coating mainly adopts dispersion method, namely utilizes the method for chemical reaction to synthesize nanometer or non-nano polyaniline particle, and recycling stirring or ultrasonic method are dispersed in the polyaniline particle in basic resin and form electrically conducting coating.
Certainly, there are some problems equally in layer/polyaniline conductive coating with this dispersion method preparation, not dispersed not good enough in coating of polyaniline particle, nano polyaniline is easily reunited, make polyaniline be difficult to distributions with nanoparticle in coating, therefore, affect to a certain extent the conductive effect of coating.
Disclose a kind of nano polyurethane antistatic coating and preparation method thereof through patent retrieval patent CN01140216.4 and formed compound system by nano-polyurethane coating and conducting powder, the nano-polyurethane coating for preparing is joined in the mica conducting powder, stir, grind, namely make the nano-polyurethane antistatic coating, wherein nano-polyurethane coating accounts for the 65-88 weight part, and conducting powder accounts for the 12-35 weight part.
CN201010548579.7 discloses a kind of water-based two-component acrylic acid polyurethane automobile paint and preparation method thereof, by A component and the preparation of B component, wherein, the A component is by the water-based hydroxyl resin of formula ratio, wetting agent, defoamer, thickening material, coupling agent, film coalescence aid add and disperse in deionized water to make in 15 minutes; The B component is polyisocyanate curing agent, takes the B component according to formula ratio, under dispersion state, the B component is slowly added in the A component, continues to disperse 5 minutes, and get final product.
CN201010562424.9 urethane cures acrylate resin antifogging abrasion resistant coating and preparation method thereof the invention discloses a kind of urethane cures acrylate resin antifogging abrasion resistant coating and preparation method thereof, urethane cures acrylate resin antifogging abrasion resistant coating is to adopt the component that comprises following mass parts to prepare: 130～190 parts of hydrophilic acrylate's resins, 210～525 parts of dead front type polyethers isocyanate curing agents, 2.00～5.00 parts of catalyzer dibutyl tin laurates.
Described patent application adds the electro-conductive material that increases the weight of umber by nano-polyurethane coating, improve anti-static effect.
Simultaneously, coating by the compound preparation of urethane cures acrylate resin two-component polymer, the method of applied chemistry mutually runs through two or more polymkeric substance and forms the netted novel complex phase polymer materials of class that interweaves, and ipn technology is the compound new technology of polymkeric substance.In the IPN material, two kinds of different reticulated structures run through mutually, and the machinery winding forms macroscopic view evenly upper, the co-mixing system of possibility phase-splitting on microcosmic.
Obviously, aniline is the dispersion method polymerization in acrylate resin, there be the dispersed not good enough problem of polyaniline particle in coating, the problem that nano polyaniline is easy to reunite is particularly appeared suddenly, nanoparticle after reunion is difficult to disperse, and makes its difficulties in dispersion in matrix resin inhomogeneous with dispersion, when carrying out simultaneously the mechanical stirring dispersion, the shape of Nano particles of polyaniline and structure are easy to destroyed, thereby affect its conductivity; Polyaniline is difficult to the distributions with nanoparticle in coating, urethane is infiltrated with it the two component polyreactions of row mutually, it is the electrically conducting coating by the compound preparation of urethane cures acrylate resin two-component polymer, two components form inierpeneirating network structure, can not have good dispersion effect between two-phase in system, thereby further affect the conductive effect of coating.
Summary of the invention
Purpose of the present invention is exactly the problem that occurs in order to solve prior art, provides a kind of nano polyaniline of in-situ emulsion polymerization preparation-epoxy acrylic resin mixture, with polyurethane two-component interpenetrating(polymer)networks Antistatic Paint and preparation method.
The present invention has developed on the one hand, and the nano polyaniline particle is uniformly dispersed in coating, make coating have electroconductibility preferably, two kinds of networks run through the interpenetrating(polymer)networks polyurethane coating that formation has conductivity mutually on the other hand, effectively control and regulate the Antistatic Paint of the mechanical property of coating by the proportioning of controlling the polyolefine network.
The present invention solves its technical problem by the following technical solutions: a kind of two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network conduction, antistatic coating, mainly that this coating is to be prepared into after being mixed by two-pack nano polyaniline-epoxy acrylic resin mixture A, base polyurethane prepolymer for use as B, wherein:
The weight ratio of A component and B component is A: B=1: 0.5～4;
By weight percentage, the content of A component is as follows:
Aniline 2-5%
Epoxy acrylic resin 4-10%
Ammonium persulphate 5-10%
Witco 1298 Soft Acid 12-18%
Water 30-45%
Dimethylbenzene 20-30%
The content of B component is as follows:
Organic solvent 10-20%
Vulcabond 15-35%
Viscotrol C 40-60%
Stablizer 1-5%
Described Viscotrol C and vulcabond weight ratio are 1: 0.3～0.7.
The organic solvent of described B component is one or more in toluene, dimethylbenzene, acetone, ethyl acetate, butylacetate, methylethylketone.
The stablizer of described B component is organotin or lead.
The vulcabond of described B component is any in 2,4 toluene diisocyanate, diphenylmethanediisocyanate, HDI.
The preparation method of a kind of two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network conduction, antistatic coating, after nano polyaniline-epoxy acrylic resin mixture A, base polyurethane prepolymer for use as B mixed, stir, standing 10-60 minute, with its brushing or be sprayed on different base materials and solidify, can obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating after 1-4 hour under room temperature.
Described A component be by aniline under the effect of doping agent and oxygenant, take epoxy acrylic resin, dimethylbenzene, water as reaction medium, carry out in-situ emulsion polymerization, react under condition of ice bath and obtained in 4～8 hours.
The doping agent of described A component is Witco 1298 Soft Acid, and oxygenant is ammonium persulphate.
Add the stirrings such as vinyl monomer, catalyzer, stopper, photostabilizer, oxidation inhibitor and filler to obtain mixture A after the repurity of described A component, drying, wherein, by weight percentage:
The vinyl monomer of described A component is one or more in vinylbenzene, methyl methacrylate, butyl methacrylate, vinyl cyanide, acrylic or methacrylic acid.
And initiator is benzoyl peroxide or Diisopropyl azodicarboxylate; Catalyzer is one or more in dibutyl tin dilaurate, stannous octoate, triethylamine, triethylene diamine; Stopper is Resorcinol, para benzoquinone, tert-butyl o biphenol.
And, photostabilizer and oxidation inhibitor are four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, Octabenzone, 2-(2-hydroxyl-3,5-two fourth uncles base phenyl)-5-chlorinated benzotriazole, (2-(2-hydroxyl-3, the 5-di-tert-pentyl-phenyl) benzotriazole, two (1,2,2,6,6-pentamethyl--4-piperidyl) one or more in sebate.
Filler is one or more in calcium carbonate, sodium carbonate, mica powder wilkinite, talcum powder, barite, and filler is dried at the temperature of 60-120 ℃ and obtained in two hours.
And the B component is to add Viscotrol C in organic solvent and vulcabond, and under drying conditions, room temperature reaction is 1～3 hour, add again initiator, stablizer and organic solvent, stirring obtains, and under 100～120 ℃ of Viscotrol C, 0.08MPa vacuum tightness, decompression dehydration obtained in 1～2 hour.
The present invention compared with prior art has the following advantages:
1, utilize polyaniline to have conductivity preferably, stable and thermostability is high in air, and quality is light, and synthesis technique is simple, synthesize the characteristics such as with low cost, take full advantage of this characteristic of polyaniline when the present invention prepares coating as a kind of comparatively desirable conductive additive.
2, adopt the method for in-situ emulsion polymerization, make aniline polymerization in epoxy acrylic resin, form the nano polyaniline particle, and be evenly dispersed in resin, the in-situ emulsion polymerization of aniline in epoxy acrylic resin is to be the mixture that medium obtains nano polyaniline and epoxy acrylic resin by oxygenant ammonium sulfate for, doping agent and emulsifying agent Witco 1298 Soft Acid, water, it be the dissemination, the oxygenant effect that utilize emulsifying agent impel aniline basic resin directly in formation nano polyaniline particle.Prepare in this way the nano polyaniline particle, can control easily and regulate on the one hand the particle diameter of nano polyaniline, prepare satisfactory nano polyaniline particle; Resin has played package action preferably to the nano polyaniline that forms on the other hand, and effectively stops the reunion of nanoparticle, and the nano polyaniline particle for preparing is dispersed in basic resin preferably, strengthens the consistency of polyaniline particle and resin.
3, utilizing ipn technology is the polymkeric substance compounding technology.aniline is in the letex polymerization of epoxy acrylic resin situ, form the nano polyaniline particle, be evenly dispersed in resin, mix with the Castor Oil PU performed polymer that contains terminal isocyanate groups, under the effect of free initiator, two key generation Raolical polymerizables in two keys in epoxy acrylic resin and Castor Oil PU form the polyolefine network, terminal isocyanate groups forms the urethane network by absorbing airborne water (moisture), polyaniline is dispersed in the Viscotrol C inierpeneirating network structure uniformly, be convenient to film forming, have conductivity and certain mechanical property preferably, two kinds of networks run through the interpenetrating(polymer)networks polyurethane coating that formation has conductivity mutually.
4, coating of the present invention combines in-situ emulsion polymerization technology, nanotechnology and polymer interpenetration network technology preferably, can solve well nano polyaniline particle dispersion problem in coating on the one hand, makes coating have electroconductibility preferably; Can also by controlling and regulate the formula of resin and additive, control easily and regulate the mechanical property of coating on the other hand.
5, the present invention utilizes epoxy acrylic resin, vinyl monomer, the Castor Oil PU performed polymer etc. that contains terminal isocyanate groups is as linking agent, makes cross-linking system contain simultaneously two keys and end group urethane.Copolymerization or the self-polymeric reaction of two keys in epoxy acrylic resin, vinyl monomer and Viscotrol C can either occur in this cross-linking system, form the polyolefine network, can utilize again to contain remaining isocyano suction (moisture) reaction formation urethane network in end group isocyanic ester Castor Oil PU performed polymer.Simultaneously, use Viscotrol C to make linking agent, enlarged the cross-linker molecules chain, improved the low temperature flexibility of filming, vinyl monomer is made linking agent and can be improved the apparent condition of filming and regulate coating performance.
6, utilize the preparation method of the electrically conducting coating that the present invention develops, gained two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network Electrical Conductivity of Conductive Coating can be stablized, can control simultaneously the add-on regulating resistance sizes values of polyaniline, regulate the mechanical property of coating by the proportioning of controlling the polyolefine network, in coating, polyaniline is uniformly dispersed, surface gloss is good, wear-resisting wiping, weather resistance is good, set time is adjustable, and the gentle hardness of filming is adjustable, and processing unit is simple, easy to operate, be conducive to industrial mass production.
Embodiment
The present invention is further described below in conjunction with embodiment.
The nano polyaniline of in-situ emulsion polymerization preparation-epoxy acrylic resin mixture, prepare coating with the polyurethane two-component interpenetrating(polymer)networks and have electroconductibility, its resistance value within the specific limits, two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network conduction antistatic coating has conduction or anti-static function.
Embodiment one:
By weight percentage, nano polyaniline-epoxy acrylic resin mixture 30%, base polyurethane prepolymer for use as (TDI) 30%, vinyl monomer 38%, catalyzer 0.5%, stopper 0.5%, photostabilizer 0.5%, initiator 0.5% stirs, obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating, under room temperature, coating is brushed or is sprayed on sheet glass and solidify.On sheet glass, the coating surface drying time is 4 hours, solidifies to record resistance value in two days and be about 5 * 105 Ω.
Embodiment two:
By weight percentage, nano polyaniline-epoxy acrylic resin mixture 13%, base polyurethane prepolymer for use as (TDI) 50%, vinyl monomer 35%, catalyzer 0.5%, stopper 0.5%, photostabilizer 0.5%, initiator 0.5% stirs, obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating, under room temperature, coating is brushed or is sprayed on sheet glass and solidify.On sheet glass, the coating surface drying time is 4 hours, solidifies to record resistance value in two days and be about 3 * 107 Ω.
Embodiment three:
By weight percentage, nano polyaniline-epoxy acrylic resin mixture 8%, base polyurethane prepolymer for use as (TDI) 56%, vinyl monomer 35%, catalyzer 0.5%, stopper 0.5%, photostabilizer 0.5%, initiator 0.5% stirs, obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating, under room temperature, coating is brushed or is sprayed on sheet glass and solidify.On sheet glass, the coating surface drying time is 4 hours, solidifies to record resistance value in two days and be about 5 * 108 Ω.
Embodiment four:
By weight percentage, nano polyaniline-epoxy acrylic resin mixture 15%, base polyurethane prepolymer for use as (HDI) 48%, vinyl monomer 35%, catalyzer) 0.5%, stopper 0.5%, photostabilizer 0.5%, initiator 0.5% stirs, obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating, under room temperature, coating is brushed or is sprayed on sheet glass and solidify.On sheet glass, the coating surface drying time is 4 hours, solidifies to record resistance value in two days and be about 1 * 108 Ω.
Claims (12)
1. a two-pack nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating network conduction, antistatic coating, it is characterized in that: this coating is to be prepared into after being mixed by two-pack nano polyaniline-epoxy acrylic resin mixture A, base polyurethane prepolymer for use as B, wherein:
The weight ratio of A component and B component is A: B=1: 0.5～4
By weight percentage, the content of A component is as follows:
Aniline 2-5%
Epoxy acrylic resin 4-10%
Ammonium persulphate 5-10%
Witco 1298 Soft Acid 12-18%
Water 30-45%
Dimethylbenzene 20-30%
The content of B component is as follows:
Organic solvent 10-20%
Vulcabond 15-35%
Viscotrol C 40-60%
Stablizer 1-5%
Described Viscotrol C and vulcabond weight ratio are 1: 0.3～0.7.
2. coating according to claim 1, it is characterized in that: the organic solvent of described B component is one or more in toluene, dimethylbenzene, acetone, ethyl acetate, butylacetate, methylethylketone, stablizer is organotin or lead.
3. coating according to claim 1 is characterized in that: the vulcabond of described B component is any in 2,4 toluene diisocyanate, diphenylmethanediisocyanate, HDI.
4. the preparation method of a two-pack nano polyaniline-epoxy acrylic resin as claimed in claim 1/polyurethane interpenetrating network conduction, antistatic coating, it is characterized in that: after nano polyaniline-epoxy acrylic resin mixture A, base polyurethane prepolymer for use as B mixed, stir, standing 10-60 minute, with its brushing or be sprayed on different base materials and solidify, can obtain two-pack nano polyaniline-epoxy acrylic resin and polyurethane interpenetrating network antistatic coating after 1-4 hour under room temperature.
5. the preparation method of coating according to claim 4, it is characterized in that: described A component be by aniline under the effect of doping agent and oxygenant, take epoxy acrylic resin, dimethylbenzene, water as reaction medium, carry out in-situ emulsion polymerization, react under condition of ice bath and obtained in 4～8 hours.
6. the preparation method of coating according to claim 5, it is characterized in that: the doping agent of described A component is Witco 1298 Soft Acid, oxygenant is ammonium persulphate.
7. the preparation method of coating according to claim 5, it is characterized in that: add the stirrings such as vinyl monomer, catalyzer, stopper, photostabilizer, oxidation inhibitor and filler to obtain mixture A after the repurity of described A component, drying, wherein, by weight percentage:
8. the preparation method of coating according to claim 7, it is characterized in that: the vinyl monomer of described A component is one or more in vinylbenzene, methyl methacrylate, butyl methacrylate, vinyl cyanide, acrylic or methacrylic acid.
9. coating according to claim 7, it is characterized in that: the initiator of described A component is benzoyl peroxide or Diisopropyl azodicarboxylate; Catalyzer is one or more in dibutyl tin dilaurate, stannous octoate, triethylamine, triethylene diamine; Stopper is Resorcinol, para benzoquinone, tert-butyl o biphenol.
10. the preparation method of coating according to claim 7, it is characterized in that: the photostabilizer of described A component and oxidation inhibitor are four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, Octabenzone, 2-(2-hydroxyl-3,5-two fourth uncles base phenyl)-5-chlorinated benzotriazole, (2-(2-hydroxyl-3, the 5-di-tert-pentyl-phenyl) benzotriazole, two (1,2,2,6,6-pentamethyl--4-piperidyl) one or more in sebate.
11. the preparation method of coating according to claim 7, it is characterized in that: the filler of described A component is one or more in calcium carbonate, sodium carbonate, mica powder wilkinite, talcum powder, barite, and filler is dried at the temperature of 60-120 ℃ and obtained in two hours.
12. the preparation method of coating according to claim 4, it is characterized in that: described B component is to add Viscotrol C in organic solvent and vulcabond, under drying conditions, room temperature reaction is 1～3 hour, add again initiator, stablizer and organic solvent, stir and obtain, and under 100～120 ℃ of Viscotrol C, 0.08MPa vacuum tightness, decompression dehydration obtained in 1～2 hour.
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| CN 201110387930 CN103131319A (en) | 2011-11-25 | 2011-11-25 | Bi-component nanometer polyaniline-epoxy acrylic resin/polyurethane interpenetrating network electric conduction and antistatic coating and preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754388A (en) * | 2016-03-02 | 2016-07-13 | 湖北启利新材料股份有限公司 | Double-component nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating-polymer-network conductive anticorrosive coating |
| CN105778750A (en) * | 2016-03-02 | 2016-07-20 | 湖北启利新材料股份有限公司 | Method for preparing double-component nano polyaniline-epoxy acrylate resin/polyurethane interpenetrating network conductive anticorrosive paint |
| CN106047070A (en) * | 2016-07-14 | 2016-10-26 | 温州乐发教育科技有限公司 | Anti-corrosion conductive polyaniline paint |
| CN106221513A (en) * | 2016-08-19 | 2016-12-14 | 仪征祥源动力供应有限公司 | A kind of preparation method of stainless steel tube antistatic coating |
| CN107474717A (en) * | 2017-08-31 | 2017-12-15 | 无锡厚发自动化设备有限公司 | A kind of host computer anti-static coatings |
| CN109705710A (en) * | 2018-12-18 | 2019-05-03 | 湖北启利新材料股份有限公司 | A kind of preparation method of antistatic aqueous finishing varnish |
-
2011
- 2011-11-25 CN CN 201110387930 patent/CN103131319A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754388A (en) * | 2016-03-02 | 2016-07-13 | 湖北启利新材料股份有限公司 | Double-component nano polyaniline-epoxy acrylic resin/polyurethane interpenetrating-polymer-network conductive anticorrosive coating |
| CN105778750A (en) * | 2016-03-02 | 2016-07-20 | 湖北启利新材料股份有限公司 | Method for preparing double-component nano polyaniline-epoxy acrylate resin/polyurethane interpenetrating network conductive anticorrosive paint |
| CN106047070A (en) * | 2016-07-14 | 2016-10-26 | 温州乐发教育科技有限公司 | Anti-corrosion conductive polyaniline paint |
| CN106221513A (en) * | 2016-08-19 | 2016-12-14 | 仪征祥源动力供应有限公司 | A kind of preparation method of stainless steel tube antistatic coating |
| CN106221513B (en) * | 2016-08-19 | 2019-04-19 | 仪征祥源动力供应有限公司 | A kind of preparation method of stainless steel tube antistatic coating |
| CN107474717A (en) * | 2017-08-31 | 2017-12-15 | 无锡厚发自动化设备有限公司 | A kind of host computer anti-static coatings |
| CN109705710A (en) * | 2018-12-18 | 2019-05-03 | 湖北启利新材料股份有限公司 | A kind of preparation method of antistatic aqueous finishing varnish |
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Application publication date: 20130605 |